Determination of phenolic compounds in medicinal preparations by galvanostatic coulometry

In this work, the possibility of using reactions of electrogenerated titrants with phenolic compounds was studied and a method for their coulometric determination in medicaments by galvanostatic coulometry was developed. The research objects were: rutin, salicylic acid and drugs containing phenolic compounds such as «Ascorutin», «Salicylic Paste» and «Salicylic Ointment» of Russian manufacture. Electrogenerated halogens (Cl2, Br2 and I2) and hexacyanoferrate(III)-ions were used as titrants. It was found that for the quantitative determination of phenolic acids, the optimal reagent is electrogenerated bromine, for rutin - electrogenerated bromine and iodine, and for ascorbic acid - any of the studied electrogenerated titrants (Cl2, Br2, I2 and [Fe(CN)6]3-). The correct definition was checked by the «entered-found» method, the error does not exceed 2%. As experimental studies have shown, our method of coulometric titration with electrogenated bromine and iodine is characterized by good reproducibility of results, expression, accuracy and can be used to determine phenolic compounds in drugs, for example, «Ascorutin» tablets. It should be noted that by our procedure it is possible to determine the spectrum of phenol-containing compounds (rutin, ascorbic and salicylic acids) in drugs without their preliminary separation. Therefore, the coulometric method using electrogenerated titrants can be recommended for the determination of salicylic, ascorbic acids and rutin in dosage forms. The proposed method is accurate and eliminates the experiment error in comparison with the Pharmacopoeic method.

Determination of low chlorine content in organic compounds and polymers using an «Expert-006» coulometer

A method of visual mercurimetric titration of chloride ions is widely used in elemental microanalysis for determination of chlorine content in organic substances after their combustion in an oxygen-filled flask. However, when chlorine content is less than 0.5%, the mercurimetric method fails to provide essential accuracy, and a more sensitive method of chlorine coulometric titration by electrogenerated silver ions appeared favorable. We consider a possibility of determining the microgram content of chloride-ions in solutions using a digital coulometric analyzer («Expert-006» produced by «Econics-Expert» (Moscow)) supplemented with an electrolytic cell with silver electrodes. The coulometer was tested in different operation modes to select the optimal electrochemical parameters of ion chloride titration and develop a technique for coulometric determination of chloride ions which in combination with the preliminary burning of the analyzed substances in an oxygen-filled flask provides determination of the residual chlorine in organic matrices at a level of 0.1 – 0.5%. The proposed technique was used to determine the residual chlorine in a number of polymers. The relative error did not exceed 5% at chlorine concentrations of 0.16 – 0.28%.

Cyclic voltammetry of natural flavonoids on MWNT-modified electrode and their determination in pharmaceuticals

The determination of rutin, quercetin and taxifolin in pharmaceutical dosage forms using cyclic voltammetry on multi-walled carbon nanotube modified glassy carbon electrode (MWNT-GCE) has been developed. The surface of the electrode created has been characterized by atomic force microscopy. Electrode modification with MWNT increases the surface average roughness (190-fold) and structures it. There are two oxidation steps at 0.22 and 0.80, 0.23 and 0.80, 0.26 and 0.86 V on cyclic voltammograms of taxifolin, quercetin and rutin, respectively, in phosphate buffer solution of pH 7.4. The linear dynamic range is 1.4–28 and 28–210, 2.0–220 and 0.52–210 μM with detection limits of 0.71, 1.0 and 0.26 μM for rutin, quercetin and taxifolin, respectively. The relative standard deviation of flavonoids determination in pharmaceuticals does not exceed of 7%. The data obtained are in good agreement with coulometric determination.